反応 #2139608

ord-6b041978ae9e45b8b118931145febe12

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONThe addition
  2. 2
    その他was exothermic to 60°
  3. 3
    抽出extracted with methylene chloride
  4. 4
    洗浄The combined extracts were washed with water
  5. 5
    乾燥dried with anhydrous MgSO4
  6. 6
    ろ過filtered
  7. 7
    濃縮concentrated

実験手順

To a stirred solution containing 34.5 g (0.20 mole) of 4-chloro-3-nitroaniline and 24 g (0.30 mole) of isopropyl mercaptan in 200 ml of DMSO was added dropwise at ambient temperature a solution of 8.0 g (0.20 mole) of sodium hydroxide in 10 ml of water. The addition was exothermic to 60° and the mixture became deep red in color. After three days, the reaction mixture was poured into water and extracted with methylene chloride. The combined extracts were washed with water, dried with anhydrous MgSO4, filtered and concentrated to give 41.1 g (97%) of product as a red-brown syrup.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04184867uspto-grants-1980_01